CN103482604A - Microwave superheated water vapor preparation method for bamboo fiber nano carbon particles - Google Patents
Microwave superheated water vapor preparation method for bamboo fiber nano carbon particles Download PDFInfo
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- CN103482604A CN103482604A CN201310428020.4A CN201310428020A CN103482604A CN 103482604 A CN103482604 A CN 103482604A CN 201310428020 A CN201310428020 A CN 201310428020A CN 103482604 A CN103482604 A CN 103482604A
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Abstract
The invention discloses a microwave superheated water vapor preparation method for bamboo fiber nano carbon particles. The method comprises the following steps of sieving of bamboo powder, pretreatment, ball milling, drying, microwave high pressure hydrothermal reaction and drying. The bamboo fiber nano carbon particles prepared through the preparation method has the characteristics of high specific surface area, high pore volume, smooth surfaces, small bore diameters, high purity and the like, more reactive groups are formed on the surfaces, and the reaction activity is high; the preparation method is simple, large scale production is facilitated, and remarkable economic and social benefits are achieved.
Description
Technical field
The invention belongs to the nano-carbon material preparation field, be specifically related to a kind of microwave superheated vapour preparation method of bamboo fiber nano carbon particle.
Background technology
Bamboo fibers tradition carbonization method complex process, surface functional group are few, and the production process energy consumption is high, can't meet the requirement of environmental protection and sustainable development.
Summary of the invention
The object of the present invention is to provide a kind of microwave superheated vapour preparation method of bamboo fiber nano carbon particle, the bamboo fiber nano carbon particle made has the characteristics such as high-specific surface area, high pore volume, smooth surface, aperture are little, high purity, surface has more reactive group, and reactive behavior is high; The preparation method is simple, is conducive to large-scale production, possesses significant economic and social benefit.
For achieving the above object, the present invention adopts following technical scheme:
A kind of microwave superheated vapour preparation method of bamboo fiber nano carbon particle comprises the following steps: the bamboo powder sieves, pre-treatment, ball milling, oven dry, microwave high pressure hydro-thermal reaction, oven dry.Concrete steps are as follows:
(1) the bamboo powder is crossed the sieve that screen-aperture is 0.15mm, standby;
(2) the bamboo powder after sieving is processed with the mixing solutions of hydrogen peroxide and urea, removed impurity, washing, dry, and obtains bamboo powder robust fibre;
(3) get 30g bamboo powder robust fibre and be placed in ball mill, adding dehydrated alcohol is dispersion medium, grinds 3 hours, obtains the bamboo fiber powder;
(4) 90 ℃, bamboo fiber powder is dried 6 hours;
(5) the bamboo fiber powder transfer after drying is to 275-320 ℃ of constant temperature 2-7 hour in the sealed pressure vessel of vapor-nozzle and running gear, naturally cooling, and 90 ℃ of oven dry 12 hours, obtain fluffy black powder, i.e. the bamboo fiber nano carbon particle.
The method directly will be reacted the ultrahigh-temperature steam jet of design temperature on raw material, because the molecule of water vapor is less, can arrive raw material inside through raw material powder, at the abrupt release high temperature of liquefaction, thereby make the heat-up time of raw material extremely short.In the time of heating, through small droplets and the residue water vapor of raw material, by the container bottom fan, discharge.Because hemicellulose and carbohydrate contained in the polysaccharide derivates in carbonization and bamboo fibers all belong to water-soluble small molecules, therefore can be taken away by water vapor and small droplets, amount discharge container, without removing impurity through washing again, and because the little cause of stream molecule can be taken away soluble impurity more up hill and dale.
Remarkable advantage of the present invention is:
(1) the bamboo fiber nano carbon particle made has the characteristics such as high-specific surface area, high pore volume, smooth surface, aperture are little, high purity, and surface has more reactive group, and reactive behavior is high.
(2), by controlling steam temperature, can make reaction carry out under condition of different temperatures, thereby obtain the nano carbon particle of different-grain diameter.
(3) preparation method is simple, is conducive to large-scale production, possesses significant economic and social benefit.
The accompanying drawing explanation
The scanning electron microscope (SEM) photograph that Fig. 1 is bamboo fiber nano carbon particle of the present invention.
Fig. 2 is the structural representation of the present invention with the sealing load device of vapor-nozzle and running gear.In figure: 1-encloses container, 2-high-temperature water vapor producer, 3-magnetic valve, 4-industrial computer, 11-temperature sensor, 12-vibrator, 13-water shoot, 131-water valve, 21-water tank, 22-electric heater, 23-steam output pipe road, 231-vapor-nozzle.
Embodiment
embodiment 1
A kind of microwave superheated vapour preparation method of bamboo fiber nano carbon particle comprises the following steps: the bamboo powder sieves, pre-treatment, ball milling, oven dry, microwave high pressure hydro-thermal reaction, oven dry.Concrete steps are as follows:
(1) the bamboo powder is crossed the sieve that screen-aperture is 0.15mm, standby;
(2) the bamboo powder after sieving is processed with the mixing solutions of hydrogen peroxide and urea, removed impurity, washing, dry, and obtains bamboo powder robust fibre;
(3) get 30g bamboo powder robust fibre and be placed in ball mill, adding dehydrated alcohol is dispersion medium, grinds 3 hours, obtains the bamboo fiber powder;
(4) 90 ℃, bamboo fiber powder is dried 6 hours;
(5) the bamboo fiber powder transfer after drying is to 275 ℃ of constant temperature in the sealed pressure vessel of vapor-nozzle and running gear 7 hours, naturally cooling, 90 ℃ of oven dry 12 hours, obtain fluffy black powder, be the bamboo fiber nano carbon particle, particle diameter is 110-120nm, productive rate 30%.
embodiment 2
A kind of microwave superheated vapour preparation method of bamboo fiber nano carbon particle comprises the following steps: the bamboo powder sieves, pre-treatment, ball milling, oven dry, microwave high pressure hydro-thermal reaction, oven dry.Concrete steps are as follows:
(1) the bamboo powder is crossed the sieve that screen-aperture is 0.15mm, standby;
(2) the bamboo powder after sieving is processed with the mixing solutions of hydrogen peroxide and urea, removed impurity, washing, dry, and obtains bamboo powder robust fibre;
(3) get 30g bamboo powder robust fibre and be placed in ball mill, adding dehydrated alcohol is dispersion medium, grinds 3 hours, obtains the bamboo fiber powder;
(4) 90 ℃, bamboo fiber powder is dried 6 hours;
(5) the bamboo fiber powder transfer after drying is to 320 ℃ of constant temperature in the sealed pressure vessel of vapor-nozzle and running gear 2 hours, naturally cooling, 90 ℃ of oven dry 12 hours, obtain fluffy black powder, be the bamboo fiber nano carbon particle, particle diameter is 100-110nm, productive rate 40%.
embodiment 3
A kind of microwave superheated vapour preparation method of bamboo fiber nano carbon particle comprises the following steps: the bamboo powder sieves, pre-treatment, ball milling, oven dry, microwave high pressure hydro-thermal reaction, oven dry.Concrete steps are as follows:
(1) the bamboo powder is crossed the sieve that screen-aperture is 0.15mm, standby;
(2) the bamboo powder after sieving is processed with the mixing solutions of hydrogen peroxide and urea, removed impurity, washing, dry, and obtains bamboo powder robust fibre;
(3) get 30g bamboo powder robust fibre and be placed in ball mill, adding dehydrated alcohol is dispersion medium, grinds 3 hours, obtains the bamboo fiber powder;
(4) 90 ℃, bamboo fiber powder is dried 6 hours;
(5) the bamboo fiber powder transfer after drying is to 300 ℃ of constant temperature in the sealed pressure vessel of vapor-nozzle and running gear 5 hours, naturally cooling, 90 ℃ of oven dry 12 hours, obtain fluffy black powder, be the bamboo fiber nano carbon particle, particle diameter is 50-70nm, productive rate 60%.
With reference to figure 2, sealing load device with vapor-nozzle and running gear, comprise the encloses container 1 and the high-temperature water vapor producer 2 that are built-in with temperature sensor 11 and vibrator 12, described high-temperature water vapor producer 2 comprises water tank 21, for electric heater 22 and the steam output pipe road 23 of heating water, described steam output pipe road 23 is connected with encloses container 1 epicoele, described steam output pipe road 23 is provided with magnetic valve 3, described temperature sensor 11 is connected with industrial computer 4 input terminuss, and described industrial computer 4 is controlled respectively electric heater 22 and magnetic valve 3 work.
In order to discharge the liquid water formed by water vapor after the interior spray bamboo fiber of encloses container 1 powder, described encloses container 1 bottom is provided with water shoot 13, and described water shoot is provided with water valve 131.
In order to monitor in real time the water temperature in encloses container, temperature sensor 11 for detecting temperature also is installed in encloses container 1, described vibrator 12 is placed in the encloses container bottom, described temperature sensor 11 is positioned at vibrator 12 tops, described vibrator 12 is at the interior left and right of encloses container 1 double vibrations, and vibrator 12 upper surfaces become the circular arc table top of indent, so that high-temperature water vapor fully sprays on bamboo fiber, make the abundant carbonization of bamboo fiber powder, carbonization is more even.
Described electric heater 22 is microwave heater.
The water vapor that hot water in the present invention after electric heater 22 heating forms rises to water tank 21 epicoeles, steam output pipe 23 input terminuss are located to water tank 21 epicoele sidewalls, so that water vapor is along steam output pipe 23 outputs, described steam output pipe 23 output terminals are provided with vapor-nozzle 231, make the water vapor of output spray more uniformly on the bamboo fiber powder, accelerate the bamboo fiber powder and form nano carbon particle.The temperature of simultaneous temperature sensor 11 real-time testing encloses container 1 interior water vapors, in order to inform industrial computer 4, allows industrial computer 4 regulate the heating power of electrically heated 22 devices, if the water temperature height reduces heating power, water temperature is hanged down the heating power that raises.Industrial computer 4 is controlled magnetic valve 3 in order to regulate in real time the work output of water vapor simultaneously.
During use, will be through the bamboo fiber powder transfer of pre-treatment to vibrator 12, by industrial computer 4 opening electric heaters 22, make the water in water tank 21 be heated to preset temperature formation high-temperature steam, opens solenoid valve 3 allows high-temperature steam pass through steam output pipe road 23 and vapor-nozzle 231 ejections, and the bamboo fiber powder vibrates to realize being heated evenly at vibrator 12 upper surfaces, continues 2-7 hour post-drying, can obtain fluffy black powder, i.e. the bamboo fiber nano carbon particle.
The foregoing is only preferred embodiment of the present invention, all equalizations of doing according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (2)
1. the microwave superheated vapour preparation method of a bamboo fiber nano carbon particle is characterized in that: comprise the following steps: the bamboo powder sieves, pre-treatment, ball milling, oven dry, microwave high pressure hydro-thermal reaction, oven dry.
2. the microwave superheated vapour preparation method of bamboo fiber nano carbon particle according to claim 1, it is characterized in that: concrete steps are as follows:
(1) the bamboo powder is crossed the sieve that screen-aperture is 0.15mm, standby;
(2) the bamboo powder after sieving is processed with the mixing solutions of hydrogen peroxide and urea, removed impurity, washing, dry, and obtains bamboo powder robust fibre;
(3) get 30g bamboo powder robust fibre and be placed in ball mill, adding dehydrated alcohol is dispersion medium, grinds 3 hours, obtains the bamboo fiber powder;
(4) 90 ℃, bamboo fiber powder is dried 6 hours;
(5) the bamboo fiber powder transfer after drying is to 275-320 ℃ of constant temperature 2-7 hour in the sealed pressure vessel of vapor-nozzle and running gear, naturally cooling, and 90 ℃ of oven dry 12 hours, obtain fluffy black powder, i.e. the bamboo fiber nano carbon particle.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104962295A (en) * | 2015-06-23 | 2015-10-07 | 湖南长笛龙吟竹业有限公司 | Bamboo carbonizing and drying integrated device and bamboo carbonizing and drying method |
| CN106833697A (en) * | 2017-01-25 | 2017-06-13 | 北京凯风泰智能技术研究有限公司 | A kind of carbon composite preparation method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1415790A (en) * | 2002-12-13 | 2003-05-07 | 东华大学 | Method for preparing bamboo fiber from bamboo |
| CN101134568A (en) * | 2007-09-19 | 2008-03-05 | 傅方堃 | Activated char activating devices and methods thereof |
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- 2013-09-18 CN CN201310428020.4A patent/CN103482604B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1415790A (en) * | 2002-12-13 | 2003-05-07 | 东华大学 | Method for preparing bamboo fiber from bamboo |
| CN101134568A (en) * | 2007-09-19 | 2008-03-05 | 傅方堃 | Activated char activating devices and methods thereof |
Non-Patent Citations (2)
| Title |
|---|
| DANIEL SCHNEIDER等: "Characterization of biochar from hydrothermal carbonization of bamboo", 《INTERNATIONAL JOURNAL OF ENERGY AND ENVIRONMENT》 * |
| WEI-HSIN CHEN 等: "Hydrothermal carbonization of sugarcane bagasse via wet torrefaction in association with microwave heating", 《BIORESOURCE TECHNOLOGY》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104962295A (en) * | 2015-06-23 | 2015-10-07 | 湖南长笛龙吟竹业有限公司 | Bamboo carbonizing and drying integrated device and bamboo carbonizing and drying method |
| CN104962295B (en) * | 2015-06-23 | 2016-12-14 | 湖南长笛龙吟竹业有限公司 | A kind of bamboo wood carbonization, the integrated device of drying and method thereof |
| CN106833697A (en) * | 2017-01-25 | 2017-06-13 | 北京凯风泰智能技术研究有限公司 | A kind of carbon composite preparation method |
| CN106833697B (en) * | 2017-01-25 | 2019-10-01 | 北京凯风泰智能技术研究有限公司 | A kind of carbon composite preparation method |
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